Process of treating distillers&#39; wash.



No. 669,8I2. Patented Mar. I2, |901. C. G. SUDRE & C. V. THIERRY. PROCESS 0F TREATING DISTILLERS WASH.

Appximion med Feb. 15, 1900., (No Model.)

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(Application filed Feb. `15, 1900.)

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UNITED STATES PATENT V OFFICE.

CHARLES GABRIEL SUDRE AND CHARLES VICTOR THIERRY, OF PARIS, FRANCE.

PROCESS OF TREATING DISTILLERS WASH.

SPECIFICATION forming part 0f Letters Patent 0. 669,812, dated March 12, 1901.

Application tiled February 15, 1900. Serial No. 5 ,355. (No specimens.)

.To all whom, if; may concern;

Be it known'that we, CHARLES GABRIEL SUDRE, residing at 12 Boulevard St. Marcel, and CHARLES VICTOR THIERRY, residing at 1l Rue Meynadier, Paris, France, citizens of the French Republic, have invented a new and useful Process of Treating Distillers Wash, of which the following is a specification.

1t is known that the residues obtained from the distillation of wines, molasses, grains, beet-roots, potatoes, and in general the residues from the distillation of all materials which have undergone an alcoholic fermentation contain glycerin, compounds of nitrogen, mineral substances, especially potash, and the like. Numerous methods have already been proposed for treating these residues with a View to obtaining as by-products of distillation glycerin, compounds of nitrogen, especially in the form of ammonia, tars, and salts.

In order to more clearly explain the nature of our invention, We refer to the accompanying drawings, illustrating one form of an apparatus or plant suitable for carrying out our process. In said drawings both gures are diagrammatic.

Figure 1 is an elevation, partly in section, showing one retort, condenser, and corresponding piping. Fig. 2 isa plan View, partly in section, showing four retorts with their proper condensers and piping.

lt will be noticed that the figures do not correspon-d with each other, as it is easier to comprehend the invention by this mode of illustration.

The Washes concentrated from 30 to 35 Baume and saturated or not with lime are introduced into a retort or cylindrical cast-iron vessel A, Fig. l. The cover of the retort has a hole a, through which passes a tube b, which descends to about one-third of the height of the retort and is drilled with a number of small openings. The upper portion of the tube b projects beyond the cover and is fitted with a three-Way cock c, so as to put it into communication either with the exterior airr or witha steam-pipe. The retort has also an outlet a', branched onto a main pipe d, fitted with valves d in such a manner that the esl thing but water'.

caping gases may be directed either to Wellknown ammonia-condensing apparatuses e e (scrubbers, purifiers, snfuric-acid tank) or to glycerin-condensers composed of carefullysealed cast-iron vessels f f, cooled by a water circulation g. The glycerin-condensers are connected to a vacuum-pump h, which is started when necessary to keep a vacuum in the glycerin-condensers and in the retort. The non-condensed gases and vapors aspirated by the pump are forced by it into the first circuit of the ammonia and tar condensers e, mentioned above, through the pipe d2. At the outlet of the last sulfuric-acid tank is placed a Roots suction-fan t, as in all gas-works. When running, the fan produces a slight vacuum or depression in the whole of the condensing apparatuses and in the retort, which helps the gases and vapors to pass through them. The fan sends the non-condensable gases into the chimney Z, Fig. 2.

It Will be observed, as shown in Fig. 2, that the retorts are in groups of four, in order to economize fuel and to utilize the same battery of condensers for the four. The reasons for this arrangement will be given later on.

The operation is conducted as follows as reugards one of the retorts: `Distilling is commenced, the air and steam entrance tube b, Fig. l, being closed, up to a temperature of about 1l()o centigrade. This hardly gives any- The retort is in connection with the ammonia and tar condensers e e. The heating is then carried progressively up to about 2Q()o centigrade, taking care to let in atmospheric air to carry o the substances produced by decomposition bet-Ween these limits of temperature and which are notably simple or compound ammonias and light tars. To let in the air, the three-way cock c, mentioned above, is opened, and the depression produced by the fan placed at the end of the condenser-battery draws in the atmospheric air, The opening of the three-way cock is so regulated that about one cubic meter of air passes per minute, which is suiiicient to carry oi the gases and vapors. During this operation the glycerin naturally is not distilled at all. When the substances decomposed toward 200 centigrade are expelled, the temperature is let fall to about 150 centigrade,

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so that the mass is partly solidified, which is useful to prevent excessive foaming when the Vacuum is applied, as will be explained. Connection is then made with the glycerincondensers f f and also with the vacuumpump h, which is then started. The threeway cock cis carefully shut. When a vacu um of about twenty millimeters of mercury is reached, the temperature is again raised toward 200 centigrade. During this period of distilling in vacuum below 200 centigrade the glycerin is distilled and at the same time a small amount of ammonia and of tar isobtained. When the glycerin is aboutexhausted, the three-way cock is turned so as to connect with the steam-pipe. The last Vestiges of glycerin in the retort are thus swept away. Then the vacuum is cut off and also the connection with the glycerin-condensers. The communication with the ammonia and tar condensers is restored. The retort is then gradually heated up to 500 or 600 centigrade until all the aminonias and heavy tars have been expelled. The only substances then left in the retort are carbonate and sulfate of potash, carbon, and impurities. The sulfate of potash comes from the combination of the potash contained in all worts undergoing fermentation with sulfuric acid, which is added to render the worts acid and so prevent the injurious non-ethylic fermentations, (lactic, butyric.) 'The proportions of sulfate of potash and of carbon are such that owing to the presence of carbon the sulfate may be transformed at very small cost into carbonate, which is at present of greater value. By this process has been obtained, on the one hand, a liquid rich in glycerin and containing a small quantity of tars and ammonias and, on the other-hand, ammoniacal and tarry liquids analogous to those coming from gas-works. These two liquids are submitted separately to the following operations: First, they are allowed to rest in cisterns or tanks. The tars being of less specific gravity rise to the surface and are skimmed or decanted. Second, the remaining liquids are passed separately through the well-known ammonia,

is sent to the ammonia-condensing columns.

The retorts are grouped in fours in the same furnace, because there are four phases in the distilling process, which correspond to four states of increasing temperature- 21e., heating at 110 centigrade, heating at 200 centigrade withv air-current, heating at 200 centigrade under Vacuum, and heating at 500 to 600 centigrade under a slight depression produced by the fan. Consequently the retort which is to be heated to 500 or 600 is the only one submitted directly to the heat of the furnace. The hot gases circulate afterward around the retorts, which should be less heated, and heat them gradually, being conducted to the chimney after the last one. Dampers le, Fig. 2, are so arranged as to facilitate this maneuver. Any one of the retorts may be isolated at will. This is done to reduce the temperature from 200 to 150. ing of coal is eifected.

The operation varies but very slightly Whatever may be the nature of the Wort, whether coming from grain,beetroot, potatoes,&c. ,for the constituents of any kind of wash arewater, glycerin, compounds of nitrogen, albuminous pecticsubstances, and mineral matters. The proportions will vary iuaccordance with the original wash; but the five constitutive principles are always the same. Consequently the duration of the phases of the operation and the quantity of products obtained will Vary, but themethod of conducting the operation Will'be invariable. The most notable difference in the products will be in the mineral residue, which in some cases may be worthless.

Having now particularly described and ascertained the nature ofour said invention and in what manner the same is tobe performed, we declare that vwhat we claim is The improved processfor treating 'the distillers wash of any materials which have undergone an alcoholic fermentation, with a View to obtaining as by-products of distillation, glycerin, compounds of nitrogen, tars and salts-which consists in previously concentrating and preferably neutralizing the residue; heating themafterward, in presence of an atmospheric air-current up to about 200 so as to Wholly evaporate the Water and collect some ammonia and light tars; in heating them -a second time up to 200 but in a Vacuum,.so as to collect the glycerin, some ammonia and the remainder of the light tars; and in removing the Vacuum and heating from 200 up to about 600 so as to collect the remainder of the am monia and the heavy tars; the residue being a mixture of carbonate and sulfate of potassium, carbon and impurities.

In testimony whereof we have signed our names to this specification in the presence of two subscribing Witnesses..

CHARLES GABRIEL SUDRE. CHARLES VICTOR THIERRY.

Witnesses:

' JULES EMILE FAYOR,

EDWARD P. MACLEAN.

By this means a notable sav- IOO IIO 

